Masakazu Horie, Moe Watanabe, Atsuko Tada, Kyoko Sato
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引用次数: 0
摘要
建立了一种简便、可靠的测定食品中泛酸的分析方法。高蛋白食品,2 g样品中加入20 mL水,匀浆提取后,加入1 mL 15%硫酸锌溶液,混合均匀,离心,过滤上清制成试验溶液。对于低蛋白食品,取20 mL 1%甲酸溶液加入2 g样品中,匀浆、提取、离心,过滤上清制成试验溶液。以0.02 mol/L磷酸盐溶液(pH 3.0)-乙腈(95:5)为流动相,采用L-柱2 ODS柱进行高效液相色谱分离,在200 nm处检测。采用L-柱2 ODS为分离柱,5 mmol/L甲酸铵(含0.01%甲酸)-甲醇(85∶15)为流动相,多重反应监测(MRM)进行检测。奶粉和营养食品中泛酸的回收率可达88%以上,精密度高。通过对市售的标记为含泛酸的食品进行分析,得到的分析值与标记值几乎一致,且HPLC法与LC-MS/MS法的分析值具有高度的相关性。
[Analysis of Free Pantothenic Acid in Foods by HPLC and LC-MS/MS].
A simple and reliable analytical method has been developed for the determination of pantothenic acid in food. For the high-protein food, 20 mL of water was added to 2 g of sample, and after homogenization extraction, 1 mL of 15% zinc sulfate solution was added, mixed well, centrifuged, and the supernatant was filtered to make the test solution. For the low-protein food, 20 mL of 1% formic acid solution was added to 2 g of sample, homogenized, extracted, centrifuged, and the supernatant was filtered to make the test solution. The HPLC separation was carried out on a L-column2 ODS column with 0.02 mol/L phosphate solution (pH 3.0)- acetonitrile (95 : 5) as the mobile phase, and detected at 200 nm. The LC-MS/MS conditions were L-column2 ODS as the separation column, 5 mmol/L ammonium formate (containing 0.01% formic acid)-methanol (85 : 15) as the mobile phase, and multiple reaction monitoring (MRM) was used for detection. The recoveries of pantothenic acid in milk powder and nutritional food products were more than 88% with high precision. As a result of analyzing commetrcially available foods labeled as containing pantothenic acid, analytical values almost identical to the labeled values were obtained, and a high correlation was observed between the values obtained by HPLC and LC-MS/MS.